CN101906044B - Synthesizing 2,5-dichloronitrobenzene by using santochlor extracted from solid waste chlorobenzene tar - Google Patents
Synthesizing 2,5-dichloronitrobenzene by using santochlor extracted from solid waste chlorobenzene tar Download PDFInfo
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- CN101906044B CN101906044B CN 201010256556 CN201010256556A CN101906044B CN 101906044 B CN101906044 B CN 101906044B CN 201010256556 CN201010256556 CN 201010256556 CN 201010256556 A CN201010256556 A CN 201010256556A CN 101906044 B CN101906044 B CN 101906044B
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Abstract
The invention mainly discloses 2,5-dichloronitrobenzene synthesized by using santochlor extracted from solid waste chlorobenzene tar. The 2,5-dichloronitrobenzene is characterized in that the solid waste chlorobenzene tar is rectified to extract low concentration santochlor, and santochlor with the concentration of 98% is extracted by a subzero crystallizing process; the santochlor is subject to a nitratlon reaction with concentrated nitric acid under the action of concentrated sulfuric acid serving as a catalyst; waste acid is separated from the product by using density contrast to obtain crude product 2,5-dichloronitrobenzene; and finally, the crude product is neutralized by using caustic soda to ensure the 2,5-dichloronitrobenzene is in slight alkalinity, and the crude product is cleaned and separated with water to obtain the pure product 2,5-dichloronitrobenzene. The invention has the advantages of not only effectively utilizing the solid waste chlorobenzene tar, contributing to environmental protection, being friendly to environment, and being capable of be produce high-purity 2,5-dichloronitrobenzene.
Description
Technical field
The present invention relates to a kind of 2, the synthesis technique of 5-dichloronitrobenzene, specifically a kind of technique of utilizing synthetic 2, the 5-dichloronitrobenzene of santochlor that extracts in the solid waste chlorobenzene coke tar.
Background technology
Utilize distillation technology to process solid waste chlorobenzene coke tar, isolate the lower concentration santochlor, through Freeze crystallization, obtain the finished product santochlor, because the solid waste chlorobenzene coke tar quality is lower, the santochlor that causes separation of produced to go out is second-rate, be in particular in that santochlor content is low, remain on about 97% shade deviation, easily lump, and wherein contain a large amount of trace impurities.Utilize this material to produce 2 by nitrated technology, the technological method of 5-dichloronitrobenzene and common chlorination process produce 2, the method of 5-dichloronitrobenzene is different, mainly be because the raw material santochlor of nitration reaction extracts from solid waste chlorobenzene tar, wherein contain a large amount of trace impurities, inhibited to subsequent reactions, therefore normal material proportion and processing condition are not enough to guarantee to react completely, and need to change proportioning and technique.
The not relevant waste that utilizes carries out the synthetic technique of 2,5-dichloronitrobenzene at present.
Summary of the invention
Main task of the present invention is to provide a kind of technique of utilizing synthetic 2, the 5-dichloronitrobenzene of santochlor that extracts in the solid waste chlorobenzene coke tar, specifically a kind ofly can utilize scrap feed material, can obtain again highly purified 2, the synthetic technology of 5-dichloronitrobenzene.
In order to solve above technical problem, a kind of santochlor synthetic 2 that extracts in the solid waste chlorobenzene coke tar that utilizes of the present invention, the 5-dichloronitrobenzene, it is characterized in that: solid waste chlorobenzene tar is carried out rectification process, extract the lower concentration santochlor, extracting content with cryogenic crystallization technique again is 98% santochlor; Then santochlor is done at the vitriol oil to carry out nitration reaction with concentrated nitric acid under the effect of catalyzer; Utilize density difference to carry out spent acid and product separation, obtain crude product 2, the 5-dichloronitrobenzene thereafter; Neutralize with caustic soda at last, make 2,5-dichloronitrobenzene slightly be alkalescence, last water cleans, separates, and obtains sterling 2, the 5-dichloronitrobenzene.
Further, in the described rectification working process, utilize single tower distillation to be combined from solid waste chlorobenzene tar dna purity with crystallization phases at the santochlor more than 99.8%, concrete steps are as follows: when a, rectification process, the middle component of cutting boiling point between Benzene Chloride and santochlor obtains the rich santochlor of santochlor purity about 75%; B, the rich santochlor with about 75% carry out centrifugal treating to the santochlor of crystallization again through the cryogenic crystallization processing, obtain purity at the santochlor more than 98%.
Further, in the described nitration reaction, the concentration of the vitriol oil is 90%
Further, in the described nitration reaction, concentration of nitric acid is 98%.
Further, the temperature of described nitration reaction is 60 ℃, treats that nitric acid reaction is complete, after santochlor reacts completely, temperature is controlled at 68～72 ℃ is incubated, and guarantees to react completely.
Further, in the described caustic soda and after 2,5-dichloronitrobenzene ph value is 12-13.
Further, the described vitriol oil: concentrated nitric acid: the mol ratio of santochlor=1: 1: 1.
The invention has the advantages that: utilize distillation technology separation and Extraction from solid waste chlorobenzene tar to go out the lower concentration santochlor, the recycling crystallizer technology is purified the lower concentration santochlor and is the high density santochlor, the high density santochlor that utilization obtains is under the katalysis of the vitriol oil, react with concentrated nitric acid, obtain highly purified 2, the 5-dichloronitrobenzene.This technique has namely effectively been utilized solid waste chlorobenzene tar, is beneficial to environmental protection, with environmental friendliness, can produce again highly purified 2, the 5-dichloronitrobenzene.
Embodiment
Implementation step of the present invention is: solid waste chlorobenzene tar is processed, extracted the lower concentration santochlor, recycling cryogenic crystallization technology extracts the high purity santochlor.Do at the vitriol oil under the effect of catalyzer, utilize concentrated nitric acid and santochlor to carry out nitration reaction, obtain high purity 2, the 5-dichloronitrobenzene.
Concrete steps are: utilize the physical synthesis integrated technology that solid waste chlorobenzene tar is carried out pre-treatment, this is treated to conventional filtration, gravity settling, material moisture from, neutralization, dry this series of steps so that through the solid waste chlorobenzene tar of pre-treatment be valuable, can directly advance tower and carry out the useful raw material that separating-purifying is processed.Above-mentioned steps is as follows:
1. utilize strainer that solid waste chlorobenzene tar is processed, remove the part solid impurity;
2. the material of step in 1. passed into gravity settling equipment, under the effect of little heating, stirring, make the solid impurity that is suspended in the material of step in 1. settlement separate;
3. the material of step in 2. passed into strainer, the thorough solid impurity among the separation of material B;
4. the material of step in 3. passed into the material water separation equipment, cutting out partial water and upper strata suspension;
5. the material of step in 4. passed into the alkali moisture eliminator, and in and contained acid in the material, make material acidity qualified;
6. the material of step in 5. passed into drying tower, obtain the material that moisture content is conventional content;
7. through separating integrated technology solid waste chlorobenzene tar is carried out pre-treatment, obtain valuablely, can directly carry out the solid waste chlorobenzene tar of the pure liquid state of rectifying separation.The ph value of the solid waste chlorobenzene tar of the described pure liquid state that obtains is 7, and water content can directly enter the raw material that rectifying tower is processed below 0.05%.
Rectification process in rectifying tower is multitower serial connection rectification process, and its concrete technology is as follows:
1. raw material is pumped into the # tower and carry out rectification process, boiling point is lower than the light constituent of santochlor, obtains the rich santochlor of santochlor purity about 85%;
2. about 85% rich santochlor being processed through cryogenic crystallization (according to difference on fusing point of, orthodichlorobenzene (53 ℃ of santochlor, orthodichlorobenzene-17 ℃), adopts the cryogenic crystallization method to separate.We are from actual production, through a large amount of research work, rich santochlor are delivered to freezer, and control freezing temp-10 ℃ finally obtains the thick santochlor of crystal 98%.Obtain purity at the santochlor more than 98%;
Next, carry out nitration reaction: preparation 90% vitriol oil 2.5t is as catalyzer and be preset in the reactor, in reactor, drop into santochlor 3t, utilize 98% nitric acid 1.35t to carry out nitrated, the control temperature treats that nitric acid reaction is complete, after santochlor reacts completely at 60 ℃, the control temperature is incubated at 68-72 ℃, guarantees to react completely.Utilize density difference to carry out spent acid and product separation thereafter, because 2, the density of 5-dichloronitrobenzene is 1.43, spent acid density is about 1.7, leaves standstill product and spent acid natural layering 15 minutes after insulation finishes, behind the discharging spent acid, obtain crude product 2, the 5-dichloronitrobenzene, neutralize with caustic soda 60kg at last, make 2,5-dichloronitrobenzene slightly be alkalescence, the ph value is in 1213, utilize at last water to clean, separate, obtain purity and be 99.5% sterling 2,5-dichloronitrobenzene 3.84t.
Claims (6)
1. one kind is utilized the santochlor synthetic 2 that extracts in the solid waste chlorobenzene coke tar, the method of 5-dichloronitrobenzene, concrete steps are: utilize the physical synthesis integrated technology that solid waste chlorobenzene tar is carried out pre-treatment, this is treated to conventional filtration, gravity settling, the material moisture from, neutralization, dry this series of steps, directly carried out the solid waste chlorobenzene tar of the pure liquid state of rectifying separation, the pH value of the solid waste chlorobenzene tar of described pure liquid state is 7, water content is below 0.05%, it is characterized in that: solid waste chlorobenzene tar is carried out rectification process, extract the lower concentration santochlor, extract again the santochlor of 98% purity with cryogenic crystallization technique; Then santochlor is done at the vitriol oil to carry out nitration reaction with concentrated nitric acid under the effect of catalyzer; Utilize density difference to carry out spent acid and product separation, obtain crude product 2, the 5-dichloronitrobenzene thereafter; Neutralize with caustic soda at last, make 2,5-dichloronitrobenzene slightly be alkalescence, last water cleans, separates, and obtains sterling 2, the 5-dichloronitrobenzene;
Rectification process in rectifying tower is multitower serial connection rectification process, and its concrete technology is as follows: 1. raw material is pumped into tower and carry out rectification process, boiling point is lower than the light constituent of santochlor, obtains the rich santochlor of santochlor purity about 85%;
2. about 85% rich santochlor is processed through cryogenic crystallization, adopted the cryogenic crystallization method to separate, rich santochlor is delivered to freezer, control freezing temp-10 ℃ obtains the thick santochlor of crystal 98%, obtains purity at the santochlor more than 98%.
2. the method for utilizing synthetic 2, the 5-dichloronitrobenzene of the santochlor that extracts in the solid waste chlorobenzene coke tar according to claim 1, it is characterized in that: in the described nitration reaction, the concentration of the vitriol oil is 90%.
3. the method for utilizing synthetic 2, the 5-dichloronitrobenzene of the santochlor that extracts in the solid waste chlorobenzene coke tar according to claim 1, it is characterized in that: in the described nitration reaction, concentration of nitric acid is 98%.
4. the santochlor that extracts in the solid waste chlorobenzene coke tar that utilizes according to claim 1 synthesizes 2, the method of 5-dichloronitrobenzene, it is characterized in that: the temperature of described nitration reaction is 60 ℃, treat that nitric acid reaction is complete, after santochlor reacts completely, temperature is controlled at 68～72 ℃ is incubated, guarantee to react completely.
5. the method for utilizing synthetic 2, the 5-dichloronitrobenzene of the santochlor that extracts in the solid waste chlorobenzene coke tar according to claim 1 is characterized in that: in the described caustic soda and after 2,5-dichloronitrobenzene pH value is 12-13.
6. the method for utilizing synthetic 2, the 5-dichloronitrobenzene of santochlor that extracts in the solid waste chlorobenzene coke tar according to claim 1 is characterized in that: the described vitriol oil: concentrated nitric acid: the mol ratio of santochlor=1: 1: 1.
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| CN102358718A (en) * | 2011-09-05 | 2012-02-22 | 江苏隆昌化工有限公司 | Method for producing o-nitro-p-chloroaniline by using chloridized aromatic hydrocarbon waste as raw material |
| CN103450025A (en) * | 2013-09-18 | 2013-12-18 | 葫芦岛天启晟业化工有限公司 | Application of anti-isomer additive in 2,5-dichloronitrobenzene production nitration reaction |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1117038A (en) * | 1994-12-29 | 1996-02-21 | 浙江大学 | Synthetic process of 2,4-fluobenzene dichloride |
| CN101580456A (en) * | 2009-04-27 | 2009-11-18 | 江苏隆昌化工有限公司 | Kettle type crystallization process of paradichlorobenzene in solid waste benzene chloride tar |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1117038A (en) * | 1994-12-29 | 1996-02-21 | 浙江大学 | Synthetic process of 2,4-fluobenzene dichloride |
| CN101580456A (en) * | 2009-04-27 | 2009-11-18 | 江苏隆昌化工有限公司 | Kettle type crystallization process of paradichlorobenzene in solid waste benzene chloride tar |
Non-Patent Citations (2)
| Title |
|---|
| 二氯苯的生产技术进展;袁俊秀;《化学工业与工程技术》;20090831;第30卷(第4期);28-30 * |
| 袁俊秀.二氯苯的生产技术进展.《化学工业与工程技术》.2009,第30卷(第4期),28-30. |
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